Hydrochloric Acid → HCID 14652622, Verbindung

HRID 477833

Reaktionsgleichung

Reaktionsgleichung von HRID 477833
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:24])=[C:10]([N:14]3[CH2:19][CH2:18][O:17][CH:16]([CH2:20][NH:21]C=O)[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4]1)[CH3:2].[ClH:29].O>CO>[ClH:29].[NH2:21][CH2:20][CH:16]1[CH2:15][N:14]([C:10]2[C:11]([F:13])=[C:12]3[C:7]([C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4][N:3]3[CH2:1][CH3:2])=[CH:8][C:9]=2[F:24])[CH2:19][CH2:18][O:17]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 146526021-Ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

Produkt 1

HCID 14652622HCID 14652622, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 500 mg of 1-ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1 ml of concentrated hydrochloric acid, 2 ml of water and 10 ml of methanol is refluxed for 1.5 hours. The reaction mixture is concentrated under reduced pressure. The obtained crystals are washed with acetone, collected by filtration and recrystallized from dimethylformamide to give 7-[2-(aminomethyl)morpholino]-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride, melting at 276°-278° C. with decomposition.

Aufarbeitung

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. washThe obtained crystals are washed with acetone
  3. filtrationcollected by filtration
  4. customrecrystallized from dimethylformamide

Quellen und Nachweise

ORD-Eintrag
ord-1875382aeec84616b2a292f5272f54b6
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04889857

Verknüpfte Notizen

Wird geladen…